CN113584351B - Rare earth-free aluminum alloy and preparation method and application thereof - Google Patents
Rare earth-free aluminum alloy and preparation method and application thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C21/00—Alloys based on aluminium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
- C22C1/026—Alloys based on aluminium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C21/00—Alloys based on aluminium
- C22C21/06—Alloys based on aluminium with magnesium as the next major constituent
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M12/00—Hybrid cells; Manufacture thereof
- H01M12/04—Hybrid cells; Manufacture thereof composed of a half-cell of the fuel-cell type and of a half-cell of the primary-cell type
- H01M12/06—Hybrid cells; Manufacture thereof composed of a half-cell of the fuel-cell type and of a half-cell of the primary-cell type with one metallic and one gaseous electrode
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
- H01M4/46—Alloys based on magnesium or aluminium
- H01M4/463—Aluminium based
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention belongs to the technical field of aluminum-air batteries, and particularly relates to a rare earth-free aluminum alloy and a preparation method and application thereof. The rare earth-free aluminum alloy provided by the invention comprises the following element components in percentage by mass: 0.2 to 1.0 percent of Bi, 0.05 to 0.2 percent of In, 0.2 to 1.0 percent of Mg and the balance of Al. According to the invention, Bi, In and Mg are added into the aluminum matrix, a compact oxide film is damaged through a cavitation effect and a eutectic body, the resistance of the oxide film is reduced, and when the oxide film is applied to the anode of the aluminum-air battery, the electrochemical activity of the anode is improved, and further the discharge voltage and the energy density of the aluminum-air battery are improved.
Description
Technical Field
The invention belongs to the technical field of aluminum-air batteries, and particularly relates to a rare earth-free aluminum alloy and a preparation method and application thereof.
Background
The aluminum air battery is used as a novel energy battery, and is widely applied to the fields of transportation, industrial production, marine emergency equipment and the like because of the advantages of light weight, zero pollution, high specific energy, low cost, good safety and the like.
The traditional aluminum air battery adopts pure aluminum as an anode material, but the aluminum is only suitable for being used as the anode of the aluminum air battery when the purity of the aluminum reaches more than 99.999 percent, which has high requirements on the electrolytic preparation process of the aluminum and increases the cost of the battery, so the aluminum air battery usually needs to be alloyed. By adopting alloying treatment, the cost is reduced, and simultaneously, the use requirement of the aluminum air battery anode can be met.
However, at present, for aluminum alloy materials, a compact oxide film is still easily formed on the surface of the aluminum alloy material, contact between aluminum and electrolyte is blocked in electrode reaction, passivation occurs, the electrode potential is rapidly reduced, the electrochemical activity is reduced, and further the discharge voltage and the energy density are reduced. Chinese patent CN111740094A discloses an aluminum alloy, wherein rare earth element Ce is used In combination with In, Sn and Mg elements, so that the alloy has refined crystal grains, weakened polarization, and improved discharge voltage and energy density of aluminum anode plate, but rare earth element is expensive, high production cost, and limits the popularization and use of aluminum air battery.
Disclosure of Invention
The invention provides a rare earth-free aluminum alloy and a preparation method and application thereof.
In order to achieve the above purpose, the invention provides the following technical scheme:
the invention provides a rare earth-free aluminum alloy which comprises the following element components in percentage by mass: 0.2 to 1.0% of Bi, 0.05 to 0.2% of In, 0.2 to 1.0% of Mg, and the balance of Al.
Preferably, the rare earth-free aluminum alloy comprises the following element components in percentage by mass: 0.4-1.0% of Bi0.4-1.0%, 0.05-0.1% of In, 0.4-0.7% of Mg and the balance of Al.
The invention also provides a preparation method of the rare earth-free aluminum alloy, which comprises the following steps:
according to the mass ratio of the metal elements In the rare earth-free aluminum alloy, a Bi source, an In source, an Mg source and an Al source are mixed and melted to obtain a molten liquid;
and after the molten liquid is cast and molded, rolling and annealing are sequentially carried out, so that the rare earth-free aluminum alloy is obtained.
Preferably, the Al source is metallic aluminum, the Bi source is metallic bismuth, the In source is metallic indium, and the Mg source is metallic magnesium;
the purities of the metal aluminum, the metal bismuth, the metal indium and the metal magnesium are independently more than or equal to 99.99%.
Preferably, the temperature of the mixing and melting is 730-800 ℃, and the time is 15-30 min.
Preferably, the casting and molding time is 5-10 min.
Preferably, the rolling mode is cold rolling.
Preferably, the rolling is multi-pass rolling, the total rolling reduction is 60-80%, and the rolling reduction of each pass is 10-20%.
Preferably, the annealing temperature is 300-450 ℃, and the time is 3-10 h.
The invention also provides application of the rare earth-free aluminum alloy in the technical scheme or the rare earth-free aluminum alloy prepared by the preparation method in the technical scheme as an anode in an aluminum-air battery.
The invention provides a rare earth-free aluminum alloy which comprises the following element components in percentage by mass: 0.2-1.0% of Bi0.2-1.0%, 0.05-0.2% of In, 0.2-1.0% of Mg and the balance of Al. In the invention, Bi, In and Mg are added into an aluminum matrix, and the Bi and the In can generate pores In an oxide film on the surface of the aluminum matrix to reduce the resistance of the oxide film; meanwhile, Bi and In can form eutectic crystals or particles, and the eutectic crystals or particles are attached between an aluminum matrix and a surface oxide film, so that the oxide film presents a discontinuous structure, and the attachment structure between the oxide film and the aluminum matrix is damaged; the magnesium can effectively improve the strength of the aluminum alloy plate, can improve the solubility of other added elements, and can effectively improve the discharge activity. When the rare earth-free aluminum alloy provided by the invention is applied to the anode of an aluminum-air battery, the electrochemical activity of the aluminum alloy is improved under the synergistic action of all components, so that the discharge voltage and the energy density of the aluminum-air battery are improved; and the adopted raw materials do not contain rare earth elements, so that the method is simple and easy to obtain, and the production cost is reduced. The results of the examples show that the aluminum alloys obtained according to the invention are at 40mA cm-2The discharge voltage under the current density is 1.056 to 1.367V, and the energy density is 2756.8 to 3531.9Wh kg-1(ii) a At 100mA cm-2The discharge voltage at current density is 0.606-0.901V, and the energy density is 1570.0-2447.3 Wh/kg-1。
Drawings
FIG. 1 is a resistance test chart of aluminum alloys obtained in examples 3 and 4 and comparative example 1;
FIG. 2 is a polarization test chart of the aluminum alloys obtained in examples 3 and 4 and comparative example 1.
Detailed Description
The invention provides a rare earth-free aluminum alloy which comprises the following element components in percentage by mass: 0.2 to 1.0 percent of Bi, 0.05 to 0.2 percent of In, 0.2 to 1.0 percent of Mg and the balance of Al.
The rare earth-free aluminum alloy provided by the invention comprises 0.2-1.0% of Bi by mass percentage, more preferably 0.4-1.0% of Bi by mass percentage, and even more preferably 0.6-1.0% of Bi by mass percentage. In a specific embodiment of the present invention, the content of Bi is specifically 0.2%, 0.4%, 0.6%, 0.8%, and 1.0%.
The rare earth-free aluminum alloy provided by the invention comprises, by mass, 0.05-0.2% of In, more preferably 0.05-0.1%, and even more preferably 0.06-0.08%.
In the present invention, the Bi and In can generate voids In the surface oxide film of aluminum, thereby reducing the resistance of the oxide film; meanwhile, Bi and In can also form eutectic crystals or particles, and the eutectic crystals or particles are attached between the aluminum matrix and the surface oxide film, so that the oxide film presents a discontinuous structure, the attachment structure of the oxide film and the aluminum matrix is damaged, and the electrochemical activity of the aluminum alloy is improved.
The rare earth-free aluminum alloy provided by the invention comprises 0.2-1.0% of Mg, more preferably 0.4-0.7%, and even more preferably 0.5-0.6% by mass. In the invention, the Mg can effectively improve the strength of the aluminum alloy plate, can improve the solubility of other added elements and can effectively improve the discharge activity.
The rare earth-free aluminum alloy provided by the invention comprises the balance of Al in percentage by mass.
According to the invention, Bi is matched with In and Mg, and the multi-component synergistic effect is realized, so that a compact oxide film is damaged through a cavity and a eutectic, the resistance of the oxide film is reduced, alloy crystal grains are refined, when the alloy is applied to an aluminum air battery anode, polarization is weakened, the electrochemical activity of the anode is improved, the overall reaction of the battery is promoted, and the discharge voltage and the energy density of an aluminum anode plate are greatly improved.
The invention also provides a preparation method of the rare earth-free aluminum alloy in the technical scheme, which comprises the following steps:
according to the mass ratio of metal elements In the rare earth-free aluminum alloy, mixing and melting a Bi source, an In source, an Mg source and an Al source to obtain a molten liquid;
and after the molten liquid is cast and molded, rolling and annealing are sequentially carried out, so that the rare earth-free aluminum alloy is obtained.
In the present invention, all the raw materials are commercially available products well known to those skilled in the art unless otherwise specified.
According to the mass ratio of metal elements In the rare earth-free aluminum alloy, a Bi source, an In source, an Mg source and an Al source are mixed and melted to obtain molten liquid.
In the present invention, the Al source is preferably metallic aluminum, the Bi source is preferably metallic bismuth, the In source is preferably metallic indium, and the Mg source is preferably metallic magnesium. In the invention, the purities of the metal aluminum, the metal bismuth, the metal indium and the metal magnesium are preferably more than or equal to 99.99 percent independently.
In the present invention, the mixing and melting preferably includes the steps of: carrying out first melting on metal aluminum to obtain molten aluminum liquid; and adding metal bismuth, metal indium and metal magnesium into the molten aluminum liquid, and performing second melting to obtain molten liquid. In the present invention, the mixing and melting are preferably performed in a medium frequency furnace.
In the invention, the first melting temperature is preferably 730-800 ℃, more preferably 750-790 ℃, and more preferably 760-780 ℃; the time is preferably 15 to 30min, more preferably 18 to 27min, and still more preferably 20 to 25 min.
In the present invention, the temperature and time of the second melting are the same as those of the first melting, and are not described herein again. In the present invention, the metal bismuth, the metal indium and the metal magnesium are preferably used in the form of metal particles. In the invention, the addition mode of the metal bismuth, the metal indium and the metal magnesium is preferably that the metal bismuth, the metal indium and the metal magnesium are wrapped by aluminum foil and then directly pressed into molten aluminum liquid. The invention has no special requirements on the thickness of the aluminum foil, and can completely wrap the metal bismuth, the metal indium and the metal magnesium. In the present invention, the second melting is preferably performed by stirring, and the stirring condition parameters in the present invention are not particularly limited, and those well known to those skilled in the art can be used. In the invention, the metal bismuth, the metal indium and the metal magnesium are wrapped by the aluminum foil, so that the oxidation of the metal bismuth, the metal indium and the metal magnesium in the melting process can be avoided.
In the present invention, the sum of the amounts of the metal aluminum and the aluminum foil preferably corresponds to the content of the aluminum element in the rare earth-free aluminum alloy.
In the process of mixing and melting the metal aluminum, the metal bismuth, the metal indium and the metal magnesium, the invention also preferably comprises refining and deslagging. The present invention has no particular requirements for the refining and deslagging process, as is well known to those skilled in the art.
After the molten liquid is obtained, the molten liquid is cast and molded, and then rolling and annealing are sequentially carried out, so that the aluminum alloy is obtained.
In the invention, the casting molding is preferably carried out in a mold, and before the casting molding, the mold is preferably preheated, wherein the preheating temperature is preferably 200-300 ℃, more preferably 220-280 ℃, and more preferably 240-260 ℃. In the invention, the casting molding time is preferably 5-10 min, more preferably 6-9 min, and even more preferably 7-8 min. In the present invention, the casting molding is preferably performed in air. The thickness of the plate obtained after the casting molding is not specially required, and the plate can be selected according to actual needs by a person skilled in the art, and is specifically 1cm in the embodiment of the invention.
After casting forming, the invention preferably sequentially rolls and anneals the cast plate to obtain the rare earth-free aluminum alloy. In the present invention, the rolling mode is preferably cold rolling. In the invention, the rolling is preferably multi-pass rolling, and the total rolling reduction is preferably 60-80%, more preferably 65-75%, and more preferably 70%; the rolling reduction of each pass is preferably 10 to 20%, and more preferably 15 to 20%. The thickness of the plate obtained after rolling is not particularly required by the invention, and can be selected by a person skilled in the art according to actual needs, and in the specific embodiment of the invention, the thickness of the plate obtained after rolling is specifically 0.2 cm.
In the invention, the annealing temperature is preferably 300-450 ℃, more preferably 330-420 ℃, and more preferably 350-400 ℃; the time is preferably 3 to 10 hours, more preferably 4 to 9 hours, and even more preferably 5 to 8 hours. Annealing under the conditions can enable the fiber structure of the rolled aluminum alloy to grow into sub-fine grains, chemical components in the grains are more uniform, and the electrochemical performance of the aluminum alloy is improved.
The invention also provides application of the rare earth-free aluminum alloy in the technical scheme or the rare earth-free aluminum alloy prepared by the preparation method in the technical scheme as an anode in an aluminum air battery. The aluminum-air battery prepared from the aluminum alloy provided by the invention has higher discharge voltage and energy density.
In order to further illustrate the present invention, the following examples are provided to describe the rare earth-free aluminum alloy of the present invention and its preparation method and application in detail, but they should not be construed as limiting the scope of the present invention.
Example 1
Melting metal aluminum at 760 ℃ for 10min to obtain molten aluminum liquid;
adding metal bismuth, metal indium and metal magnesium wrapped by aluminum foil into molten aluminum liquid, and performing second melting under stirring at 760 ℃ for 10min to obtain molten liquid;
preheating a mould, pouring the molten liquid into the mould for casting molding after the temperature of the mould reaches 240 ℃, wherein the casting molding time is 5min, and obtaining a molded plate with the thickness of 1 cm;
cold rolling the formed plate, wherein the reduction thickness of each pass is 0.1cm, and rolling for 8 times to obtain a rolled plate with the thickness of 0.2 cm;
and annealing the rolled plate at 350 ℃ for 6h to obtain the rare earth-free aluminum alloy.
Examples 2 to 5 and comparative examples 1 to 3
An aluminum alloy was prepared according to the method of example 1, wherein the compositions of each example and comparative example are shown in table 1.
TABLE 1 compositions of aluminum alloys prepared in examples 1 to 5 and comparative examples 1 to 3
| Bi/wt％ | In/wt％ | Mg/wt％ | Al/wt％ | |
| Example 1 | 0.2 | 0.075 | 0.5 | 99.225％ |
| Example 2 | 0.4 | 0.075 | 0.5 | 99.025％ |
| Example 3 | 0.6 | 0.075 | 0.5 | 98.825％ |
| Example 4 | 0.8 | 0.075 | 0.5 | 98.625％ |
| Example 5 | 1.0 | 0.075 | 0.5 | 98.425％ |
| Comparative example 1 | 0 | 0 | 0 | 100％ |
| Comparative example 2 | 0 | 0.075 | 0.5 | 99.425％ |
| Comparative example 3 | 0 | 0.5 | 0.5 | 99.0％ |
Performance testing
The aluminum alloys obtained in examples 1 to 5 and comparative examples 1 to 3 were applied to aluminum air batteries, and the electrolyte of the aluminum air batteries was a 4mol/L NaOH aqueous solution. The obtained aluminum-air battery was subjected to a discharge performance test, and the test results are shown in table 2.
TABLE 2 test results of discharge properties of aluminum-air batteries prepared in examples 1 to 5 and comparative examples 1 to 3
From the results in Table 2, it is understood that the aluminum-air battery produced from the aluminum alloy of the present invention has a capacity of 40mA cm-2The discharge voltage under the current density is 1.056-1.367V, and the energy density is 2756.8-3531.9 Wh-kg-1(ii) a At 100mA cm-2The discharge voltage at current density is 0.606-0.901V, and the energy density is 1570.0-2447.3 Wh/kg-1。
The aluminum alloys obtained in examples 3 and 4 and comparative example 1 were subjected to the resistance test, and the test results are shown in fig. 1. As can be seen from fig. 1, the impedance curves of the aluminum alloys obtained in examples 3 and 4 and the pure aluminum of comparative example 1 show a uniform trend, i.e., two capacitive rings for high and low frequencies. However, the impedance radius of the high-frequency capacitance ring of the aluminum alloy added with the elements In, Mg and Bi is obviously smaller than that of pure aluminum, which shows that Bi dissolved In the aluminum matrix enables the anode to be refined, the resistance of the oxide film is reduced, the polarization resistance is reduced and the activity of the anode is enhanced; the addition of magnesium element can reduce hydrogen evolution corrosion and increase corrosion resistance; meanwhile, In and Bi are added into an aluminum matrix, a eutectic mixture is easily formed at high temperature, eutectic crystals or particles are formed after solidification and attached between the aluminum matrix and a surface oxide film, so that the oxide film presents a discontinuous structure, the attachment structure of the oxide film and the matrix is damaged, and the resistance of the oxide film is reduced. Under the synergistic effect of three elements of In, Mg and Bi, the crystal grains of the aluminum alloy are refined, and the electrochemical activity is improved.
The aluminum alloys obtained in examples 3 and 4 and comparative example 1 were subjected to a polarization test, and the test results are shown in fig. 2. As can be seen from fig. 2, the aluminum alloys obtained In examples 3 and 4 have a potential positive shift and an increased corrosion resistance compared to pure aluminum, which indicates that the addition of In, Mg and Bi not only further improves the activation of the anode, but also facilitates the reduction of the self-corrosion rate and the reduction of the position of the hydrogen-evolving cathode, so that the corrosion current density is significantly reduced and the activation and corrosion resistances are compatible. Under the synergistic action of In, Mg and Bi, the aluminum alloy provided by the invention shows excellent activation performance.
Although the above embodiments have been described in detail, they are only a part of the embodiments of the present invention, not all of the embodiments, and other embodiments can be obtained without inventive step according to the embodiments, and all of the embodiments belong to the protection scope of the present invention.
Claims (5)
1. The preparation method of the rare earth-free aluminum alloy is characterized by comprising the following steps of:
mixing and melting a Bi source, an In source, an Mg source and an Al source to obtain a molten liquid;
after the molten liquid is cast and molded, rolling and annealing are sequentially carried out, so that the rare earth-free aluminum alloy is obtained;
the rolling mode is cold rolling; the rolling is multi-pass rolling, the total rolling reduction is 60-80%, and the rolling reduction of each pass is 10-20%;
the annealing temperature is 300-450 ℃, and the annealing time is 3-10 h;
the rare earth-free aluminum alloy comprises the following element components in percentage by mass: 0.2 to 1.0 percent of Bi, 0.05 to 0.2 percent of In, 0.2 to 1.0 percent of Mg and the balance of Al.
2. The preparation method according to claim 1, wherein the rare earth-free aluminum alloy comprises the following element components in percentage by mass: 0.4-1.0% of Bi, 0.05-0.1% of In, 0.4-0.7% of Mg and the balance of Al.
3. The production method according to claim 1, wherein the Al source is metallic aluminum, the Bi source is metallic bismuth, the In source is metallic indium, and the Mg source is metallic magnesium;
the purities of the metal aluminum, the metal bismuth, the metal indium and the metal magnesium are independently more than or equal to 99.99 percent.
4. The preparation method according to claim 1 or 3, wherein the temperature of the mixed melt is 730-800 ℃ and the time is 15-30 min.
5. The preparation method according to claim 1, wherein the casting time is 5-10 min.
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| CN102820472B (en) * | 2012-08-07 | 2015-03-18 | 河南科技大学 | Manganese-aluminum containing anode material and preparation method thereof, as well as air cell prepared by using anode material |
| CN110190289A (en) * | 2019-07-11 | 2019-08-30 | 吉林大学 | Aluminium-air cell Al-Ga-In-Sn-Bi anode material and its preparation method and application |
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| GB1528182A (en) * | 1975-03-24 | 1978-10-11 | British Aluminium Co Ltd | Alloys |
| JP2005307251A (en) * | 2004-04-20 | 2005-11-04 | Sumitomo Light Metal Ind Ltd | Aluminum alloy clad material for automobile heat exchanger |
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